反应详情

温度

120 °C

3.84 g (7.52 mmol) of benzyl 4,4-dimethoxy-3-oxobutyrate, 1.30 ml (11.5 mmol) of 3-chlorobenzaldehyde and 0.114 ml of piperidine were heated under reflux in 11.5 ml of benzene overnight while water was removed. The reaction solution was washed with water and then dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue thus obtained and 1.77 g (11.5 mmol) of 2-cyanoethyl 3-aminocrotonate were heated at 70° C. under stirring in 57.5 ml of 2-propanol overnight. The reaction mixture was then heated at 120° C. under stirring under atmospheric pressure for 4 hours while 2-propanol was evaporated. The residue was purified by the silica gel chromatography (hexane/ethyl acetate=2/1) to obtain the title compound.

1. customwas removed
2. washThe reaction solution was washed with water
3. dry with materialdried over anhydrous magnesium sulfate
4. customThe solvent was evaporated under reduced pressure
5. customThe residue thus obtained
6. customwas evaporated
7. customThe residue was purified by the silica gel chromatography (hexane/ethyl acetate=2/1)